AFM Microscopy Research Articles

Micro structures, Morphology and Optical Properties of Sb2O3: WO3, In2O3 Nanostructure Composite Thin Films

This work is concerned with the synthesis of two types of composites thin films (Sb2O3:WO3 and (Sb2O3:In2O3) with different concentrations (0.0,0.05,0.1, and 0.15). The prepared thin films are characterized with the use of the X-ray diffraction atomic force microscope AFM and UV-Vis–infrared spectrophotometer. The structural examination shows that both composite's thin films were polycrystalline with nano size with cubic phase as majority and orthorhombic phase as minority phase. The crystal size decreases from 34.6 to 24.7 and 21.7 nm for (Sb2O3:WO3) and (Sb2O3:In2O3) thin films, respectively. The average roughness shows non-regular growth by increasing the concentration of both oxides. The optical energy band gap shows a red shift for both types of nanostructure thin films, which populate these composited thin films for solar cell applications.

Optimization of MBE-grown GaSb buffer on GaAs substrates for infrared detectors

The aim of this work was to improve the quality of the GaSb buffer layers on GaAs substrates using the molecular beam epitaxy (MBE) technology. The high quality of the GaSb buffer layers is one of the most important elements enabling the synthesis of good quality of type II superlattices (T2SL) structures for infrared applications. The main challenges in this regard are: compensation of the difference in lattice constants between GaAs and GaSb and obtaining the highest achievable surface quality of the final GaSb layer. In the literature, many authors describe different techniques to obtain the best quality of a GaSb buffer layer. In this work, we present the results of HRXRD, AFM, TOF-SIMS, SEM, and Nomarski optical microscope measurements obtained for 2 μm thick GaSb buffer layers. The GaSb layers are made according to different techniques and these results are compared with a GaSb buffer construction technique according to our own technology. During the processes, we also obtained an unintentional structure of one of the buffer layers, which allowed us to obtain very good results in terms of surface structure and crystallographic quality where FWHM in ωRC scan was equal to 138 arcsec and RMS 0.20 nm proving that there is still a lot of work to be done in this area.

Antibacterial and antibiofilm activity of human gut lactic acid bacteria.

The present study focused on the antibacterial and antibiofilm activity of novel lactic acid bacterial (LAB) strains isolated from the healthy human volunteers of different age groups and their consortium (LABCON), against the enteropathogenic bacteria. From the study, methanolic extract of LAB isolates and their consortia were found to have promising antibacterial activity and antibiofilm activity against Escherichia coli (ATCC 35218) and Staphylococcus aureus (ATCC 25923). The antimicrobial compounds including the DL-3 phenyllactic acid, DL-p-hydroxyphenyllactic acid, and Succinic acid produced by the LAB could be considered to inhibit the growth and biofilm formation by E. coli (ATCC 35218) and S. aureus (ATCC 25923). Detailed insight into the antibiofilm activity could also be demonstrated by Confocal Raman microscopy attached with AFM and Fluorescent microscope. From the results of the study, the consortium LABCON was superior in antimicrobial and antibiofilm activity and can be considered to have promising application in infection control.

Effect of inclusion complex formation and mechanoactivation on the structure and rheological behavior of starch-oleic acid mixtures

In the present work, for the first time, mechanical activation implemented in a rotor-stator device (RSD) has been used to enhance the formation of the amylоse-fatty acid complex in gelatinized starch at a moderate temperature (40 °C) using oleic acid (ОА) as a model guest compound. Mechanical activation was found to cause an increase in the complexing index from 10 to 30 % for non-activated mixtures to 83–92 %. The study of aqueous and dried starch-OA mixtures using optical and AFM microscopy and dynamic light scattering methods revealed a uniform distribution of amylose-OA complex particles with a size of 125–260 nm in the starch matrix. The freeze-dried starch-ОА sample prepared using mechanical activation exhibited a V-type crystalline structure. By rotational viscometry and dynamic rheometry, it was found that mechanical activation causes the gelation of aqueous starch-OA mixtures, which accompanies a decrease in their fluidity and an increase in elasticity. The developed method can be recommended for large-scale production of thickening and texture modifying materials based on gelatinised starch containing a fatty acid as a nutritional or structuring additive.

Thermo- and Photoresponsive Smart Nanomaterial Based on Poly(diethyl vinyl phosphonate)-Capped Gold Nanoparticles.

A new nanodevice based on gold nanoparticles (AuNPs) capped with poly(diethylvinylphosphonate) (PDEVP) has been synthesized, showing interesting photophysical and thermoresponsive properties. The synthesis involves a properly designed Yttriocene catalyst coordinating the vinyl-lutidine (VL) initiator active in diethyl vinyl phosphonate polymerization. The unsaturated PDEVP chain ending was thioacetylated, deacetylated, and reacted with tetrachloroauric acid and sodium borohydride to form PDEVP-VL-capped AuNPs. The NMR, UV-Vis, and ESI-MS characterization of the metal nanoparticles confirmed the formation of the synthetic intermediates and the expected colloidal systems. AuNPs of subnanometric size were determined by WAXD and UV-Vis analysis. UV-Vis and fluorescence analysis confirmed the effective anchoring of the thiolated PDEVP to AuNPs. The formation of 50-200 nm globular structures was assessed by SEM and AFM microscopy in solid state and confirmed by DLS in aqueous dispersion. Hydrodynamic radius studies showed colloidal contraction with temperature, demonstrating thermoresponsive behavior. These properties suggest potential biomedical applications for the photoablation of malignant cells or controlled drug delivery induced by light or heat for the novel PDEVP-capped AuNP systems.

Femtosecond laser-induced damage threshold incubation in SrTiO3 thin films

This study delved into the microfabrication process on SrTiO3 thin films using femtosecond laser pulses, focusing on characterizing ablation behavior and elucidating on incubation parameters. A combination of microscopy techniques and systematic analysis of laser-material interactions provided insights into the features and fundamental processes governing the laser-induced modification of SrTiO3 thin films. The cutting profile morphology indicated high-resolution material removal, with line widths ranging from 0.6 to 1.6 µm, depending on number of pulses and energy. The study revealed a low incubation parameter for SrTiO3 thin films, quantified as (0.03 ± 0.01), indicating that a considerable number of pulses is required to cause damage to the material. Additionally, threshold energies for damage were determined to be 17.9 nJ for 20,000 pulses and 35.2 nJ for a single pulse. AFM analysis showed that the depth of the micromachined lines increased from approximately 80 nm to 315 nm with higher pulse energies, confirming substantial material removal. The Keldysh parameter provides insights into ionization mechanisms under femtosecond-laser irradiation, highlighting the dominance of tunneling ionization. Using higher pulse energies, the center of the microstructures exhibited significantly reduced Raman signals, correlating with substantial material removal, which was confirmed by atomic force microscopy. EDS analyses indicated that the elemental composition of the irradiated regions closely resembled the stoichiometric composition of SrTiO3, while the center of the microstructures showed significant oxygen levels but lacked titanium and strontium, consistent with the findings from AFM and Raman microscopy.

Nanoscale elemental and morphological imaging of nitrogen-fixing cyanobacteria.

Nitrogen-fixing cyanobacteria bind atmospheric nitrogen and carbon dioxide using sunlight. This experimental study focused on a laboratory-based model system, Anabaena sp., in nitrogen-depleted culture. When combined nitrogen is scarce, the filamentous prokaryotes reconcile photosynthesis and nitrogen fixation by cellular differentiation into heterocysts. To better understand the influence of micronutrients on cellular function, 2D and 3D synchrotron X-ray fluorescence mappings were acquired from whole biological cells in their frozen-hydrated state at the Bionanoprobe, Advanced Photon Source. To study elemental homeostasis within these chain-like organisms, biologically relevant elements were mapped using X-ray fluorescence spectroscopy and energy-dispersive X-ray microanalysis. Higher levels of cytosolic K+, Ca2+, and Fe2+ were measured in the heterocyst than in adjacent vegetative cells, supporting the notion of elevated micronutrient demand. P-rich clusters, identified as polyphosphate bodies involved in nutrient storage, metal detoxification, and osmotic regulation, were consistently co-localized with K+ and occasionally sequestered Mg2+, Ca2+, Fe2+, and Mn2+ ions. Machine-learning-based k-mean clustering revealed that P/K clusters were associated with either Fe or Ca, with Fe and Ca clusters also occurring individually. In accordance with XRF nanotomography, distinct P/K-containing clusters close to the cellular envelope were surrounded by larger Ca-rich clusters. The transition metal Fe, which is a part of nitrogenase enzyme, was detected as irregularly shaped clusters. The elemental composition and cellular morphology of diazotrophic Anabaena sp. was visualized by multimodal imaging using atomic force microscopy, scanning electron microscopy, and fluorescence microscopy. This paper discusses the first experimental results obtained with a combined in-line optical and X-ray fluorescence microscope at the Bionanoprobe.

Application of Hipims Coatings to Enhance the Durability and Performance of Structural Components of PEM Electrolyzer Anodes

Porous transport layers (PTL) and bipolar plates (BPP) are structural elements that transport water, gases, electrons as well as heat within the electrolysis cells. On the anode side, the state-of-the-art material for BPP and PTL is titanium due its higher corrosion resistance under the operating conditions of electrolysis (high electrochemical potential, acidic and oxidizing environment) compared to other materials [1]. However, titanium components tend to form an oxide layer that rises the interfacial contact resistance (ICR) and leads to a poor performance since metal oxides are semiconductors or insulators. This issue is usually addressed by applying precious metal coatings, such as platinum or gold. In this work, we present the potential of high power sputtering techniques (HiPIMS) to manufacture ultra-low loading Pt coatings (<20 nm) with good homogeneity and high performance at an industrial scale. The influence of HiPIMS parameters on coating-substrate interface, as well as the coating properties have been evaluated. SEM, AFM and HRTEM microscopy have been used to evaluate the coating thickness and morphology. XRD analysis has been carried out to evaluate the influence of the HiPIMS parameters on the growth mode of Pt coatings, tailoring the coating texture from [200] to [111]. HiPIMS technique also provide enhanced density compared with other coating techniques due to the higher ionization achieved in the plasma [2]. The deposition of denser and defect-free coatings by HiPIMS enables the application of stainless steel components. HiPIMS prevents the formation of columnar structures and reduces oxygen diffusion. In this work, Nb- and Ti-based protective coatings have been deposited by HiPIMS on stainless steel 316L. A comparative between coated Ti Gr2 and SS316L has been set, showing the potential to reduce costs in the next generation of PEMWE structural components.

Photocatalytic coatings with self-cleaning properties for indoor air treatment

In this work we have studied the photocatalytic and self-cleaning properties of TiO2 layers immobilized on polymeric panels, as passive elements for air treatment. In order to achieve easy scale-up technologies for the preparation of coatings, roller-coating technique was selected, comparing the results with those prepared by dip-coating. Composites were characterized by SAXRD, UV–Vis DRS spectroscopy, profilometry, N2 adsorption–desorption, SEM and AFM microscopy. The adherence of the coating was evaluated according the ASTM D3359 standard adhesive tape test. The photocatalytic properties of the materials were evaluated by the photodegradation of trichloroethylene or formaldehyde, as model volatile organic compounds, in the gas phase. The hydrophilic-hydrophobic properties were measured by studying the in-situ variation of the water contact angle with time and UV-A irradiation. Moreover, the self-cleaning properties were analyzed according to ISO 27448:2009 for oleic acid removal. Although coatings of approximately ca. 250 nm layer thickness can be prepared by both techniques, roller-coating allows the material deposition with a coral-like structure in a single and simple step. Surface roughness was promoted by roller process. The developed materials present high photocatalytic performance for the elimination of both model pollutants in the gas phase. Aging tests under outdoor conditions and Scotch tape test show the stability and resistance of the coatings. In-situ irradiation measurements show the superhydrophilic character of the coatings. Water contact angle lower than 10 ° after 300 min of UV-A irradiation was achieved for oleic acid removal. The combination of TiO2 nanoparticles with different crystal structures and sizes improves the photocatalytic performance. A correlation between the ability for pollutants degradation in gas phase and the self-cleaning properties (in-situ or oleic acid measurements) was determined.

Heavy Metal Detection and Removal by Composite Carbon Quantum Dots/Ionomer Membranes.

The combination of ion exchange membranes with carbon quantum dots (CQDs) is a promising field that could lead to significant advances in water treatment. Composite membranes formed by sulfonated poly(ether ether ketone) (SPEEK) with embedded CQDs were used for the detection and removal of heavy metal ions, such as lead and cadmium, from water. SPEEK is responsible for the capture of heavy metals based on the cation exchange mechanism, while CQDs detect their contamination by exhibiting changes in fluorescence. Water-insoluble "red" carbon quantum dots (rCQDs) were synthesized from p-phenylenediamine so that their photoluminescence was shifted from that of the polymer matrix. CQDs and the composites were characterized by several techniques: FTIR, Raman, UV/VIS, photoluminescence, XPS spectroscopies, and AFM microscopy. The heavy metal ion concentration was analyzed by inductively coupled plasma-optical emission spectroscopy (ICP-OES). The concentration ranges were 10.8-0.1 mM for Pb2+ and 10.0-0.27 mM for Cd2+. SPEEK/rCQDs showed a more pronounced turn-off effect for lead. The composite achieved 100% removal efficiency for lead and cadmium when the concentration was below a half of the ion exchange capacity of SPEEK. The regeneration of membranes in 1 M NaCl was also studied. A second order law was effective to describe the kinetics of the process.

Using Poly(N‐isopropylacrylamide) and Poly(ethyleneglycol) Grafted Polycarbodiimides as Unique Nanocarriers for Hydrophobic Form of the Doxorubicin (DOX)

AbstractAmphiphilic helical polycarbodiimides bearing side chains with terminal alkyne groups provide a unique platform for construction of polymeric micelles. Incorporation of propargyl pendants into polyguanidine backbone allowed post‐polymerization modification with azide terminated, random coil, poly(N‐isopropylacrylamide), PNIPAM15K and poly(ethyleneglycol), PEG2K moieties using copper‐catalyzed click reaction (CuAAC). Thus, four new amphiphilic brush copolymers with varying grafting density were synthesized and their self‐assembly behavior in aqueous medium was studied by combination of TEM, SEM, AFM, and optical microscopy techniques. It was shown the formation of micellar structures at critical micelle concentration (CMC) ranging from 1.58 × 10−5 to 1.05 × 10−3mg mL−1. A hydrophobic drug doxorubicin (DOX) was then encapsulated successfully into these micellar structures with encapsulation efficiency (EE) falling in the range from 16% to 27%. Further, the cellular uptake studies were carried out by using HeLa cells and the cytotoxic activity of DOX‐loaded micelles was determined to be less than 65% of cell viability at a concentration of 0.250 mg mL−1. Fluorescence microscopy imaging revealed importing the micelles into the cells by endocytosis and internalization of the DOX into nucleus of the HeLa cells.

Modification of mono-layer MoS2 through post-deposition treatment and oxidation for enhanced optoelectronic properties

Precise control of the optical and electrical properties of mono-layer (ML) thin MoS2 is crucial for future applications in functional devices. Depending on the synthesis route and the post-deposition annealing protocols, the number of sulfur vacancies in the material is different, which has a profound impact on the properties of the 2D layer. Here, we show that the sulfur vacancy-rich ML MoS2 films oxidize already at room temperature, which changes the photoluminescence (PL) yield, the MoS2–Al2O3 substrate interaction, and the structural integrity of the films. We used x-ray photoelectron spectroscopy to monitor the formation of MoO3 and possibly MoS3−xOx after exposure to air and to quantify the number of sulfur defects in the films. Atomic force microscopy measurements allow us to pinpoint the exact regions of oxidation and develop a dedicated low temperature heating procedure to remove oxidized species, leading to MoO3-free MoS2 films. AFM and Kelvin probe force microscopy show that the MoS2–Al2O3 substrate coupling is changed. The reduction in the MoS2–substrate coupling, combined with a preferential oxidation of sulfur vacancies, leads to a sevenfold increase in the PL intensity, and the ratio between trions and neutral excitons is changed. Our work highlights the importance of oxidized sulfur vacancies and provides useful methods to measure and manipulate their number in MoS2. Furthermore, changes in the MoS2–substrate interaction via sulfur vacancies and oxidation offer an elegant pathway to tune the optoelectronic properties of the two-dimensional films.

Photochemical stability of chitosan films doped with cannabis oil

The effect of UV radiation from three different sources on chitosan (CS) films containing the addition of 10% by weight of cannabis oil was investigated. Cannabis oil (CBD) alone exposed to UV is unstable, but its photostability significantly increases in the chitosan matrix. The course of photochemical reactions, studied by FTIR spectroscopy, is slow and inefficient in chitosan with CBD, even under high-energy UV sources. The research also included chitosan films with CBD cross-linked with dialdehyde starch (DAS). Using AFM microscopy and contact angle measurements, the morphology and surface properties of prepared chitosan films with CBD were investigated, respectively. It was found that CBD embedded in CS is characterized by the best photostability under the influence of an LED emitting long-wave radiation. Using a monochromatic and polychromatic UV lamp (HPK and UV-C) emitting high-energy radiation, gradual degradation accompanied by oxidation was observed, both in the CS chains and in the CBD additive. Additionally, changes in surface properties are observed during UV irradiation. It was concluded that CS protects CBD against photodegradation, and a further improvement in photochemical stability is achieved after system cross-linking with DAS.

Enhancement of NiO/Si solar cell by adding porous silicon and a silicon dioxide SiO2 carrier selective layer

In this work, we fabricated a novel heterojunction, Silicon-based solar cell. We used nickel oxide NiO thin films on porous silicon PS separated by a thin silicon dioxide SiO2 carrier-selective layer p-NiO/(SiO2) PS/(n+) Si (Silicon). For comparison, we also manufactured a p-NiO/(n+) Si device. The Atomic Force microscopy AFM and scanning electron microscopy SEM images highlighted the nanoporous pyramidal like structures for p-NiO/(SiO2) PS/(n+) Si devices that decreased the optical reflectivity to 2 %. From the electrochemical study, low resistance and high minority carrier lifetime (1.44 ms) were estimated for p-NiO/(SiO2) PS/n+-Si. The results are promising and agree with a high power conversion efficiency of 19.52 % for p-NiO/(SiO2) PS/n+-Si versus 3.8 % for p-NiO/Si.

Performance and mechanism of graphene oxide removal from aqueous solutions by calcite: adsorption isotherms, thermodynamics, and kinetics.

The flow of graphene oxide (GO) into natural water systems can adversely affect water environments and ecosystems. In this study, the adsorption effect of calcite on GO under different conditions was studied using calcite as adsorbent. Meanwhile, characterized by a combination of microscopic experiments, including SEM, TEM, XRD, FTIR, Raman, XPS, and AFM, additional research on the performance and the mechanism of GO sorption by calcite was conducted. The findings indicated that the highest adsorption efficiency was observed at a temperature of 303 K, pH 3, a mass of 90 mg of calcite, with an initial concentration of 60 mg L-1 GO, resulting in a 95% adsorption rate. The adsorption isotherm conformed to the model of Langmuir and Temkin, and it is a heat absorption process dominated by monolayer adsorption. The thermodynamic analysis showed that the adsorption was spontaneous and heat-absorbing. The adsorption kinetics conformed to the pseudo-second-order kinetic model, and the sorption procedure is chemisorption. In conclusion, calcite has a good sorption capacity for GO, which can provide a reference for the removal of GO in the aqueous environment.

A hybrid fluorescent nanofiber membrane integrated with microfluidic chips towards lung-on-a-chip applications.

Here, we report a fluorescent electrospun nanofiber membrane for integration into microfluidic devices towards lung-on-a-chip applications complemented with the results of computational fluid dynamics modelling. A proposed hybrid poly(ε-caprolactone) (PCL)-collagen membrane was developed, characterized, tested, and integrated into a prototype microfluidic chip for biocompatibility studies. The resulting membrane has a thickness of approximately 10 μm, can be adjusted for appropriate porosity, and offers excellent biocompatibility for mimicry of a basement membrane to be used in lung-on-a-chip device applications. Several membrane variations were synthesized and evaluated using SEM, FTIR, AFM, and high-resolution confocal fluorescence microscopy. A sample microfluidic chip made of cyclic olefin copolymer and polydimethylsiloxane was built and integrated with the developed PCL-collagen membrane for on-chip cell culture visualisation and biocompatibility studies. The sample chip design was modelled to determine the optimal fluidic conditions for using the membrane in the chip under fluidic conditions for future studies. The integration of the proposed membrane into microfluidic devices represents a novel strategy for improving lung-on-a-chip applications which can enhance laboratory recapitulation of the lung microenvironment.

Heteroepitaxy in Organic/TMD Hybrids and Challenge to Achieve it for TMD Monolayers: The Case of Pentacene on WS2 and WSe2.

The intriguing photophysical properties of monolayer stacks of different transition-metal dichalcogenides (TMDs), revealing rich exciton physics including interfacial and moiré excitons, have recently prompted an extension of similar investigations to hybrid systems of TMDs and organic films, as the latter combine large photoabsorption cross sections with the ability to tailor energy levels by targeted synthesis. To go beyond single-molecule photoexcitations and exploit the excitonic signatures of organic solids, crystalline molecular films are required. Moreover, a defined registry on the substrate, ideally an epitaxy, is desirable to also achieve an excitonic coupling in momentum space. This poses a certain challenge as excitonic dipole moments of organic films are closely related to the molecular orientation and film structure, which critically depend on the support roughness. Using X-ray diffraction, optical polarization, and atomic force microscopy, we analyzed the structure of pentacene (PEN) multilayer films grown on WSe2(001) and WS2(001) and identified an epitaxial alignment. While (022)-oriented PEN films are formed on both substrates, their azimuthal orientations are quite different, showing an alignment of the molecular L-axis along the and directions. This intrinsic epitaxial PEN growth depends, however, sensitively on the substrates surface quality. While it occurs on exfoliated TMD single crystals and multilayer flakes, it is hardly found on exfoliated monolayers, which often exhibit bubbles and wrinkles. This enhances the surface roughness and results in (001)-oriented PEN films with upright molecular orientation but without any azimuthal alignment. However, monolayer flakes can be smoothed by AFM operated in contact mode or by transferring to ultrasmooth substrates such as hBN, which again yields epitaxial PEN films. As different PEN orientations result in different characteristic film morphologies (elongated mesa islands vs pyramidal dendrites), which can be easily distinguished by AFM or optical microscopy, this provides a simple means to judge the roughness of the used TMD surface.

DNA structural changes (photo)induced by tricarbonyl (pterin)rhenium(I) complex

We report on interactions of different types of DNA molecules including double-stranded and plasmid DNA as well as polynucleotides (poly[dGdC]2 and poly[dAdT]2) with fac-[ReI(CO)3(pterin)(H2O)] (or Reptr) complex. The interaction was characterized spectroscopically and changes in the plasmid structure were verified by both electrophoresis and AFM microscopy. For comparative reasons, two others related tricarbonyl rhenium(I) complexes, fac-[(4,4′-bpy)ReI(CO)3(dppz)]+ (or Redppz) and fac-[(CF3SO3)ReI(CO)3(2,2′-bpy)] (or Rebpy) were also studied to further explore the influence of the different co-ligands on the interaction and DNA (photo)damage. Data reported herein suggests that DNA molecules can be structurally modified either by direct interaction with Re(I) complexes in their ground states inducing DNA relaxation, and/or through photoinduced cross-linking processes. The chemical nature of the co-ligands modulates the extent of the damage observed.

Exploring the Local Optoelectronic Properties of ALD Grown TiO2 Photoelectrode-Coatings with Atomic Force Microscopy Methods

Photoelectrochemical cells (PECs) hold great promise as an environmentally friendly method of converting sunlight into valuable fuels. However, the semiconductor components of PEC photoelectrodes are susceptible to corrosion under photoelectrochemical conditions.In order to protect the surface of these semiconductors from degradation, a thin overlayer of Titanium dioxide (TiO2) is often applied by atomic layer deposition (ALD). In addition to their protecting function, the physicochemical properties of these thin films significantly affect the overall performance of the device. The local nano-scale optoelectronic characteristics, which considerably influence their macroscopic properties, have rarely been reported in the literature.AFM methods constitute a powerful tool to investigate photo-induced charge separation, charge transport and recombination on photoelectrode surfaces with nanometer resolution.In this context, we have employed Tunneling Conductive AFM (TUNA) and Kelvin Probe Force Microscopy (KPFM) in the dark and under illumination to investigate the surface of ALD-grown TiO2. The synthesis conditions determine the morphology, which has a strong impact on the local optoelectronic properties. TUNA measurements reveal higher photogenerated currents on the grain and facet boundaries, showing that these regions can be favorable conduction pathways. Based on KPFM experiments we can quantify the more efficient photo-induced charge separation on the crystalline TiO2 inclusions, which generate a significant surface photopotential (~450 mV) upon UV-illumination. Categorization of different regions of surface topography based on morphology allows us to analyze the evolution of surface potential over time and extract localized time constants for carrier dynamic processes on the films. This spatially resolved information provides valuable insight to guide the development of macroscopically stable and efficient photoelectrodes through the engineering of microstructure at the nano scale.

Annealing-free fabrication of high-quality indium tin oxide films for free-carrier-based hybrid metal–semiconductor nanophotonics

Recent discoveries have revealed that indium tin oxide (ITO), due to the presence of an epsilon-near-zero (ENZ) point and suitable carrier concentration and mobility, can be used to modulate the refractive index, confine fields in the nanoscale, enhance nonlinear effects, achieve ultrafast light switching or to construct so-called time-varying media. While this potential positions ITO as a key material for future nanophotonic devices, producing ITO films with precisely engineered properties remains a significant challenge. Especially when the device’s complex geometry or incorporated materials require the fabrication process to be conducted at substrate temperatures below 100 °C and without any post-annealing treatment. Here we present a comprehensive study on the low-temperature deposition of 70 nm thick ITO films using an e-beam PVD system. The nanolayers evaporated under different conditions were characterized by SEM and AFM microscopy, Hall effect measurement system as well as spectroscopic ellipsometry. We discuss the factors influencing the optical, electrical, and morphological properties of ITO films. We show that smooth nanolayers of similar quality to annealed samples can be obtained at 80 °C by controlling the oxygen plasma parameters, and the ENZ wavelength can be tuned throughout the NIR spectral range. Finally, we show that using the proposed methodology, we fabricated ITO films with resistivity as low as 5.2 × 10–4 Ω cm, smooth surface with RMS < 1 nm, high carrier concentration reaching 1.2 × 1021 cm−3 and high transmittance (85%) in the Vis/NIR spectrum.